CN106810619B - A kind of gingko episperm pectin and polypentenol extracting method - Google Patents
A kind of gingko episperm pectin and polypentenol extracting method Download PDFInfo
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Abstract
The invention discloses a kind of methods that gingko episperm extracts polypentenol and pectin simultaneously, are characterized in that: selection picks ginkgo in the Chinese olive phase；Gingko episperm is smashed to pieces after rinsing；The gingko episperm smashed to pieces leaches in leaching liquid；Leach the pectin solution activity carbon decoloring obtained；Pectin solution after decoloration is concentrated using ceramic super-filtering film；Pectin solution after concentration uses ethanol precipitation；Pectin crude extract is purified using ethyl alcohol immersion process；Pectin drying after purification, is ground into powder；The filter residue obtained after pectin extraction is leached by leaching agent of petroleum ether, and vacuum distillation obtains blackish green oily polypentenol crude extract；Polypentenol crude extract is hydrolyzed with the NaOH ethanol solution of 2-10%, is collected the progress molecular distillation of petroleum ether phase solution and is condensed into thick oil-like extracts；Polypentenol extract carries out silica gel column chromatography after using petroleum ether dissolution, and vacuum distillation obtains pale yellowish oil polypentenol sterling after the elution of petrol ether/ethyl acetate mixed liquor.
Description
Technical field
This technology is related to food and medicine field, and in particular to a kind of that polypentenol and pectin are extracted from gingko episperm
Method.
Background technique
Natural polypentenol is that one kind by isopentene group unit and terminal prenol unit polymerize the long-chain linear formed
Lipids is widely present in plant, animal, bacterium and fungi.Polyprenols From Ginkgo Biloba L is by 14-24 (with 17-19
Based on) the birch terpene alcohols polypentenol that constitutes of a isopentene group unit, with polyterpene contained in human body and mammal internal organs
Structure feature and the carbochain distribution of alcohol are very much like, and can be metabolized to dolichol phosphate ester in vivo and become sugared egg in biomembrane
The carrier of sugar when white synthesis.Polypentenol is nontoxic to the human body, without mutagenesis, teratogenesis and carcinogenesis, to promoting body hematopoiesis machine
Energy, alpastic anemia etc. have important pharmacology, drug action.Therefore, polypentenol is a kind of ginkgo that can be made full use of
The exploitation of native compound, polypentenol related drugs and health food will further promote the sustainable development of ginkgo industry
Exhibition.
Ginkgo polypentenol compound is mainly extracted from ginkgo leaf, is extracted also by gingko episperm at present
Do not report.Gingko episperm is the cortex of food containing gingko almond, i.e. seed hard shell exterior portion, is commonly called as gingko afterbirth, and quality accounts for
The 70% of entire seed.Gingko episperm complicated component has many-sided pharmacology living containing a variety of active ingredients and nutritional ingredient
Property, there is higher utility value, can be used for the exploitation of drug, health care product and plant pesticide, has broad application prospects.According to system
Meter, there are about 30,000 tons or so exospers to be dropped as waste every year in China, is not exploited, not only waste of resource but also pollution
Environment, and skin contact can also cause to paint malicious sample dermatitis.Pectin, flavones, phenolic acid etc. is extracted from gingko episperm at present to change
The report for closing object is more, and the low polar compound such as polypentenol is all dropped in extraction process, causes the very big wave of resource
Take.If made full use of by isolated polypentenol, so that it may provide more excellent drugs for the mankind, change give up into
It is precious, or vast ginkgo grower additional income.
Ginkgo polypentenol extracting method has organic solvent extraction and supercritical extraction etc., and wherein organic solvent extracts
Method due to have many advantages, such as it is easy to operate, be easy to amplify and be widely used, this method is mainly soluble in using polypentenol
The characteristics of nonpolarity such as petroleum ether, n-hexane, acetone or weak polar solvent, therefore select petroleum ether, n-hexane-acetone, acetone-
Chloroform, n-hexane-ether, methanol-acetone etc. are that Extraction solvent extracts polypentenol.But this method only extracts single non-pole
The substance of property, the substances such as water-soluble pectin are all taken as impurity treatment and fall.Pectin is the seventh-largest nutrient diet fiber of human body
Main component, have multiple eating and medical value, field of food pectin be often used as gelling agent, thickener, stabilizer,
Suspending agent, emulsifier, fumet etc.；Have reducing blood lipid, hypoglycemic, norcholesterol, weight-reducing, anti-cancer anti-in terms of Medicines and Health Product
Cancer, antiallergy, improves immunity, the pharmacological actions such as cough-relieving apophlegmatic at anti-aging, can be used for treating cardiovascula arteriosclerosis, diabetes and
The antidote of the heavy metal poisonings such as the diseases such as gastric ulcer and lead, mercury, cobalt, being also used as function controlling agent and hemostat makes
With.In conclusion exploitation good separating effect, extraction efficiency are high, solvent utilization rate is high, cost is relatively low, have industrialized production
The gingko episperm of future extracts polypentenol and pectin new process and ginkgo utilization efficiency can be improved in new method, produces for ginkgo
New life is injected in the sustainable development of industry.
Summary of the invention
The purpose of the present invention is exploitation good separating effect, extraction efficiency is high, solvent utilization rate is high, cost is relatively low, has
The gingko episperm of industrialized production future extracts polypentenol and pectin new process and new method.
Definition: gingko episperm: ginkgo is gymnosperm, is wrapped in gingko seed (gingko seed includes pulp and shell)
The part of outer similar pulp is exosper.
1, a kind of gingko episperm pectin and polypentenol extracting method, which is characterized in that in turn include the following steps:
(1) picking of ginkgo fruit
Selection picks ginkgo in Chinese olive phase (the 7-9 month), and it is spare to strip exosper；
(2) gingko episperm pre-processes
Gingko episperm first pass around screening removal go rotten, corruption raw material, it is selected after starting material with water rinse 2-5 times,
Wind drenches 5-30min, is then crushed gingko episperm using food masher；
(3) pectin leaches
The ratio of 1:5-1:30 adds leaching liquid, solute composition are as follows: phosphoric acid into the gingko episperm of crushing in mass ratio
Sodium (Na3PO4) 2-8wt%, disodium hydrogen phosphate (Na2HPO4) 0.5-4wt%, sodium citrate (Na3C6H5O7) 10-100mM, hydroxyl
Acetic acid (HOCH2COOH) 0.2-1wt%；Leaching liquid salt acid for adjusting pH value to 2-6；The stirring leaching 45- at 70-90 DEG C
120min；Leaching operation reactor is 3-8 fixed bed reactors, and using multi-stage batch counter-current extraction operating procedure, (adverse current is soaked
Process is taken to refer to that material and leaching liquid are flowed at opposite direction, material is from left side reactor reactor flow to the right, leaching
Liquid is from right side reactor reactor flow to the left)；Pectin solution is obtained using plate filter filtering after leaching；
(4) pectin solution decolourizes
Active carbon, and the 30- that decolourizes under the conditions of 50-70 DEG C of temperature are added in step (3) filtered pectin solution
The ratio of 120min, pectin solution and active carbon is 1L:5-20g；Filtering obtains pectin solution；
(5) pectin solution is concentrated
Step (4) filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, solution body after concentration
Product is the 20-50% that preceding original solution volume is concentrated, and ultrafiltration retaining molecular weight is 10,000-300,000, and operating pressure is
0.05-0.3MPa, operation temperature are room temperature；Obtain fructose concentrating liquid；
(6) pectin ethanol precipitation
The ethanol water of volumetric concentration 85-95% is added in step (5) fructose concentrating liquid, controls ethyl alcohol in mixed liquor
Final volume concentration is 50%-80%, is stirred evenly, and adjusts the pH value of mixed liquor to 3-6, standing 0.5-4 hours to be precipitated complete
After filter, solid matter be obtain pectin crude extract；
(7) pectin crude extract purifies
The pectin crude extract that step (6) obtains is purified using ethyl alcohol immersion process, and concentration of alcohol is followed successively by dehydrated alcohol, body
Product concentration 88-92% ethanol water and volumetric concentration 78-82% ethanol water, soaking temperature are room temperature, when every section of immersion
Between be 30-90min；
(8) pectin is dry
Pectin after purification is dried at 50-70 DEG C, is then comminuted into pectin powder.
(9) polypentenol leaches
The filter residue that step (3) is obtained by filtration leaches polypentenol, solid-liquid ratio 1:5-1:10, leaching by leaching agent of petroleum ether
Taking temperature is 60-90 DEG C, leaching time 60-300min；Leaching operation reactor is 3-8 fixed bed reactors, using more
(counter-current extraction process refers to that material is flowed with leaching liquid at opposite direction to grade interval counter-current extraction operating procedure, and material is from a left side
Side reaction device reactor flow to the right, leaching liquid is from right side reactor reactor flow to the left)；Plate and frame filter press filtering is received
Collect filtrate, filtrate carries out vacuum distillation concentration, distillation pressure 1,000-10, and 000Pa, temperature are 40-60 DEG C of acquisition blackish green
Oily crude extract；
(10) polypentenol crude extract hydrolyzes
The crude extract obtained in step (9) is the mixture of polypentenol He its acetic acid esters, it is necessary to be hydrolyzed and be gathered
Pentenol, hydrolyzate are the NaOH ethanol solution of 2-10%, and crude extract and hydrolyzate volume ratio are 1:5-20, and hydrolysis temperature is
50-70 DEG C, hydrolysis time 30-240min, collection petroleum ether phase solution progress molecular distillation, distillation pressure 0.5-100Pa,
30-60 DEG C of cryosurface temperature, 50-90 DEG C of circulating water temperature, 40-80 DEG C of material heating temperature, 180-320 DEG C of vapo(u)rizing temperature are received
Collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol ointment is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:2-5,
Then silica gel column chromatography is carried out；Silica gel (50-200 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:5-20
(sample/silica gel), eluent are petrol ether/ethyl acetate mixed liquor, and ratio 9:1-7:3, eluting temperature is 25-50 DEG C, is received
Collection eluent is evaporated under reduced pressure, distillation pressure 1,000-10, and 000Pa, vapo(u)rizing temperature are 40-60 DEG C, obtains light yellow oil
Shape product.
Above-mentioned gingko episperm pectin and polypentenol extracting method, step (1) are as follows: select the Chinese olive phase in ginkgo
(the 7-9 month) picking, is placed in ventilated environment storage, spare, and when processing strips exosper；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (2) are as follows: gingko episperm
First pass around screening removal go rotten, corruption raw material, it is selected after raw material rinse 3 times, wind drench 10min, then use food powder
Broken machine crushes gingko episperm；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (3) are as follows: in mass ratio 1:
The ratio of 5-1:30 adds leaching liquid, leaching liquid composition: sodium phosphate (Na into the gingko episperm of crushing3PO4) 2-8%, phosphoric acid
Disodium hydrogen (Na2HPO4) 0.5-4%, sodium citrate (Na3C6H5O7) 10-100mM, hydroxyacetic acid (HOCH2COOH) 0.2-1%.
Leaching operation reactor is 3-8 fixed bed reactors, and using multi-stage batch counter-current extraction operating procedure, (counter-current extraction process is
Refer to that material and leaching liquid are flowed at opposite direction, material is from left side reactor reactor flow to the right, and leaching liquid is from right side
Reactor reactor flow to the left)；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (4) are as follows: pectin solution is adopted
With active carbon decoloring, 50-70 DEG C of bleaching temperature, bleaching time 30-120min, the ratio of pectin solution and active carbon is 1L:5-
20g；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (5) are as follows: super using ceramics
Pectin solution is concentrated in filter membrane, and volume is the 20-50% of original solution volume after concentration, and ultrafiltration retaining molecular weight is 10,000-
300,000, operating pressure 0.05-0.3Mpa；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (6) are as follows: fructose concentrating liquid
Using ethanol precipitation pectin, the final volume concentration of ethyl alcohol is 50%-80%, and the pH of solution is 3-6, and time of repose is that 0.5-4 is small
When；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (7) are as follows: pectin crude extract
It is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by dehydrated alcohol, volumetric concentration
88-92% ethanol water and volumetric concentration 78-82% ethanol water, soaking temperature are room temperature, soaking time 30-
90min；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (8) are as follows: fruit after purification
Glue is dried at 50-70 DEG C, is then comminuted into pectin powder.
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (9) are as follows: after pectin extraction
Obtained filter residue leaches polypentenol, solid-liquid ratio 1:5-1:10 by leaching agent of petroleum ether, and leaching temperature is 60-90 DEG C, leaching
Taking the time is 60-300min；Leaching operation reactor is 3-8 fixed bed reactors, is operated using multi-stage batch counter-current extraction
(counter-current extraction process refers to that material and leaching liquid are flowed at opposite direction to technique, and material is from left side reactor side reaction to the right
Device flowing, leaching liquid is from right side reactor reactor flow to the left)；Filtrate is collected by filtration in plate and frame filter press, and filtrate is subtracted
Distillation and concentration, distillation pressure 1,000-10 are pressed, 000Pa Pa, temperature are 40-60 DEG C of acquisition blackish green oily crude extract；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (10) are as follows: polypentenol is thick
Extract uses the NaOH ethanol solution of 2-10% to be hydrolyzed for hydrolyzate, and crude extract and hydrolyzate volume ratio are 1:5-20, water
Solving temperature is 50-70 DEG C, hydrolysis time 30-240min, collects petroleum ether phase solution and carries out molecular distillation, distillation pressure is
0.5-100Pa, 30-60 DEG C of cryosurface temperature, 50-90 DEG C of circulating water temperature, 40-80 DEG C of material heating temperature, vapo(u)rizing temperature
180-320 DEG C, collection evaporates excess, obtains dark-brown polypentenol extract；
Further, above-mentioned gingko episperm pectin and polypentenol extracting method, step (11) are as follows: polypentenol is soft
Cream is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:2-5, then carries out silica gel column layer
Analysis；Silica gel (50-200 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:5-20 (sample/silica gel), elution
Liquid is petrol ether/ethyl acetate mixed liquor, and ratio 9:1-7:3, eluting temperature is 25-50 DEG C, collects eluent and is depressurized
Distillation, distillation pressure 1,000-10,000Pa, vapo(u)rizing temperature are 40-60 DEG C, obtain pale yellowish oil product.
Compared with prior art, technical solution provided by the invention has following technological merit:
(1) the characteristics of present invention chooses the Chinese olive phase (the 7-9 month) that gingko episperm is fruit, which picks is that pectin contains
Amount is high, easily stored and progress pre-treatment.
(2) technical solution provided by the invention can extract polypentenol and pectin simultaneously in gingko episperm, improve
The utilization rate of gingko resource.
(3) technical solution provided by the invention has prepared a kind of new gingko episperm pectin extraction method, in acid solution
Add sodium phosphate (Na3PO4), disodium hydrogen phosphate (Na2HPO4), calgon ((NaPO3)6) outer kind of shell, addition can be softened
Ethylenediamine tetra-acetic acid (EDTA), hydroxyacetic acid (HOCH2COOH Ca in outer kind of shell can) be chelated2+、Mg2+Plasma, to improve
Pectin extraction yield.
(4) technical solution pectin leaching provided by the invention leaches operating procedure using multi-stage countercurrent, and pectin can be improved
Extraction efficiency, while the dosage of leaching liquid can also be reduced, reduce production cost.
(5) technical solution polypentenol leaching provided by the invention leaches operating procedure using multi-stage countercurrent, can be improved
Polypentenol extraction efficiency, while the dosage of petroleum ether can also be reduced, reduce energy consumption, pollutant discharge amount and production cost.
(6) technical solution polypentenol provided by the invention is carried out pure using silica gel column chromatography and the method for molecular distillation
Change, the purity of polypentenol can reach 90% or more in final product.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but do not constitute any limitation of the invention.Anyone is within the scope of the invention as claimed
Any type of modification made, still within the claims in the present invention protection scope.
Embodiment 1
The method that a kind of gingko episperm provided by the invention extracts pectin and polypenthylene acid simultaneously successively includes following step
It is rapid:
(1) picking of ginkgo fruit
It selects to pick in the Chinese olive phase (the 7-9 month) of ginkgo, is placed in ventilated environment and stores；It is spare to strip exosper.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate (Na into the raw material of crushing in mass ratio3PO4)
3%, disodium hydrogen phosphate (Na2HPO4) 0.9%, sodium citrate (Na3C6H5O7) 50mM, hydroxyacetic acid (HOCH2COOH) 0.4%.
PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 3 fixed bed reactors, is used
Multi-stage batch counter-current extraction operating procedure；Pectin solution is obtained using plate filter filtering after leaching.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after concentration
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, the pH value for adjusting mixed liquor with hydrochloric acid (HCl) stands completely rear filtering to be precipitated in 4 hours, obtain pectin to 3.5
Crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, and every section of soaking time is 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) polypentenol leaches
It extracts the filter residue obtained after pectin and leaches polypentenol, solid-liquid ratio 1:5, leaching temperature by leaching agent of petroleum ether
It is 75 DEG C, leaching time 120min；Leaching operation reactor is 3 fixed bed reactors, using multi-stage batch counter-current extraction
Operating procedure；Plate and frame filter press is collected by filtration filtrate, and filtrate carries out vacuum distillation concentration, distillation pressure 1,000-10,
000Pa, temperature are 50 DEG C of acquisition blackish green oily crude extracts；
(10) polypentenol crude extract hydrolyzes
Polypentenol crude extract uses 5% NaOH ethanol solution to be hydrolyzed for hydrolyzate, crude extract and hydrolyzed liquid
For product than being 1:5, hydrolysis temperature is 60 DEG C, hydrolysis time 120min, collects petroleum ether phase solution and carries out molecular distillation, distillation pressure
Power is 0.5-100Pa, 35 DEG C of cryosurface temperature, 60 DEG C of circulating water temperature, 70 DEG C of material heating temperature, 280 DEG C of vapo(u)rizing temperature, is received
Collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol ointment is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:3, so
After carry out silica gel column chromatography；Silica gel (100 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:7 (sample/silicon
Glue), eluent is petrol ether/ethyl acetate mixed liquor, and ratio 8:2, eluting temperature is 30 DEG C, collects eluent and is depressurized
Distillation, distillation pressure 1,000-10,000Pa, vapo(u)rizing temperature are 50 DEG C, obtain pale yellowish oil product.
(12) it calculates recovery rate: obtaining 130 grams of jelly powders, calculate 130 grams/1000 grams of recovery rate, obtaining recovery rate is
13%；14 grams of polypentenols are obtained, calculate 14 grams/1000 grams of recovery rate, obtaining recovery rate is 1.4%.
The comparative example 1:(maturity period picks the gingko episperm of fruit, extracts pectin experiment)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, strip
Exosper is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate (Na into the raw material of crushing in mass ratio3PO4)
3%, disodium hydrogen phosphate (Na2HPO4) 0.9%, sodium citrate (Na3C6H5O7) 50mM, hydroxyacetic acid (HOCH2COOH) 0.4%.
PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 3 fixed bed reactors, is used
Multi-stage batch counter-current extraction operating procedure；Pectin solution is obtained using plate filter filtering after leaching.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after molten contracting
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, soaking time 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
9) polypentenol leaches
It extracts the filter residue obtained after pectin and leaches polypentenol, solid-liquid ratio 1:5, leaching temperature by leaching agent of petroleum ether
It is 60 DEG C, leaching time 120min；Leaching operation reactor is 3 fixed bed reactors, using multi-stage batch counter-current extraction
Operating procedure；Plate and frame filter press is collected by filtration filtrate, and filtrate carries out vacuum distillation concentration, distillation pressure 1,000-10,
000Pa, temperature are 50 DEG C of acquisition blackish green oily crude extracts；
(10) polypentenol crude extract hydrolyzes
Polypentenol crude extract uses 4% NaOH ethanol solution to be hydrolyzed for hydrolyzate, crude extract and hydrolyzed liquid
For product than being 1:5, hydrolysis temperature is 55 DEG C, hydrolysis time 120min, collects petroleum ether phase solution and carries out molecular distillation, distillation pressure
Power is 0.5-100Pa, 35 DEG C of cryosurface temperature, 60 DEG C of circulating water temperature, 70 DEG C of material heating temperature, 240 DEG C of vapo(u)rizing temperature, is received
Collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol ointment is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:3, so
After carry out silica gel column chromatography；Silica gel (100 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:5 (sample/silicon
Glue), eluent is petrol ether/ethyl acetate mixed liquor, and ratio 8:2, eluting temperature is 30 DEG C, collects eluent and is depressurized
Distillation, distillation pressure 1,000-10,000Pa, vapo(u)rizing temperature are 50 DEG C, obtain pale yellowish oil product.
(12) it calculates recovery rate: obtaining 80 grams of jelly powders.80 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is 8%；
12 grams of polypentenols are obtained, calculate 12 grams/1000 grams of recovery rate, obtaining recovery rate is 1.2%.
Comparative example 2:(traditional extraction liquid extracts pectin comparative experiments)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, it is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate (Na into the raw material of crushing in mass ratio3PO4)
3%.PH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 3 fixed bed reactors,
Using multi-stage batch counter-current extraction operating procedure；Pectin solution is obtained using plate filter filtering after leaching.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after molten contracting
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, and every section of soaking time is 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into pectin powder.
(9) polypentenol leaches
It extracts the filter residue obtained after pectin and leaches polypentenol, solid-liquid ratio 1:5, leaching temperature by leaching agent of petroleum ether
It is 55 DEG C, leaching time 60min；Leaching operation reactor is 3 fixed bed reactors, is grasped using multi-stage batch counter-current extraction
Make technique；Plate and frame filter press is collected by filtration filtrate, and filtrate carries out vacuum distillation concentration, distillation pressure 1,000-10,000Pa,
Temperature is 50 DEG C of acquisition blackish green oily crude extracts；
(10) polypentenol crude extract hydrolyzes
Polypentenol crude extract uses 4% NaOH ethanol solution to be hydrolyzed for hydrolyzate, crude extract and hydrolyzed liquid
For product than being 1:5, hydrolysis temperature is 50 DEG C, hydrolysis time 60min, collects petroleum ether phase solution and carries out molecular distillation, distillation pressure
Power is 0.5-100Pa, 35 DEG C of cryosurface temperature, 60 DEG C of circulating water temperature, 70 DEG C of material heating temperature, 240 DEG C of vapo(u)rizing temperature, is received
Collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol ointment is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:3, so
After carry out silica gel column chromatography；Silica gel (100 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:5 (sample/silicon
Glue), eluent is petrol ether/ethyl acetate mixed liquor, and ratio 8:2, eluting temperature is 30 DEG C, collects eluent and is depressurized
Distillation, distillation pressure 1,000-10,000Pa, vapo(u)rizing temperature are 50 DEG C, obtain pale yellowish oil product.
(12) it calculates recovery rate: obtaining 50 grams of jelly powders.50 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is 5%.
11 grams of ginkgolic acids are obtained, calculate 11 grams/1000 grams of recovery rate, obtaining recovery rate is 1.1%.
Embodiment 2
A kind of gingko episperm pectin provided by the invention and polypentenol extracting method, in turn include the following steps:
(1) picking of ginkgo fruit
It selects to pick in the Chinese olive phase of ginkgo, is placed in ventilated environment and stores, it is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate (Na into the raw material of crushing in mass ratio3PO4)
8%, disodium hydrogen phosphate (Na2HPO4) 1.5%, sodium citrate (Na3C6H5O7) 100mM, hydroxyacetic acid (HOCH2COOH) 1%.With
Hydrochloric acid (HCl) adjusts pH value to 2, stirs 90min at 80 DEG C.Leaching operation reactor is 4 fixed bed reactors, using more
Grade interval counter-current extraction operating procedure；Pectin solution is obtained using plate filter filtering after leaching.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 70 DEG C, pectin solution and active carbon
Ratio is 1L:10g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and liquor capacity is original after concentration
The 30% of liquor capacity, ultrafiltration retaining molecular weight are 50,000, and operating pressure 0.2MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 4, stand completely rear filtering to be precipitated in 1 hour, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, soaking time 60min.
(8) pectin is dry
Pectin after purification is dried at 65 DEG C, is then comminuted into jelly powder.
(9) polypentenol leaches
It extracts the filter residue obtained after pectin and leaches polypentenol, solid-liquid ratio 1:7, leaching temperature by leaching agent of petroleum ether
It is 75 DEG C, leaching time 120min；Leaching operation reactor is 4 fixed bed reactors, using multi-stage batch counter-current extraction
Operating procedure；Plate and frame filter press is collected by filtration filtrate, and filtrate carries out vacuum distillation concentration, distillation pressure 1,000-10,
000Pa, temperature are 50 DEG C of acquisition blackish green oily crude extracts；
(10) polypentenol crude extract hydrolyzes
Polypentenol crude extract uses 5% NaOH ethanol solution to be hydrolyzed for hydrolyzate, crude extract and hydrolyzed liquid
For product than being 1:7, hydrolysis temperature is 70 DEG C, hydrolysis time 120min, collects petroleum ether phase solution and carries out molecular distillation, distillation pressure
Power is 0.5-100Pa, 35 DEG C of cryosurface temperature, 60 DEG C of circulating water temperature, 70 DEG C of material heating temperature, 280 DEG C of vapo(u)rizing temperature, is received
Collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol ointment is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:5, so
After carry out silica gel column chromatography；Silica gel (100 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:10 (sample/
Silica gel), eluent is petrol ether/ethyl acetate mixed liquor, and ratio 8:2, eluting temperature is 30 DEG C, collects eluent and is subtracted
Pressure distillation, distillation pressure 1,000-10,000Pa, vapo(u)rizing temperature are 50 DEG C, obtain pale yellowish oil product.
(12) it calculates recovery rate: obtaining 150 grams of jelly powders.150 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is
15%.16 grams of ginkgolic acids are obtained, calculate 16 grams/1000 grams of recovery rate, obtaining recovery rate is 1.6%.
The comparative example 3:(maturity period picks the gingko episperm of fruit, extracts pectin experiment)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, it is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate (Na into the raw material of crushing in mass ratio3PO4)
8%, disodium hydrogen phosphate (Na2HPO4) 1.5%, sodium citrate (Na3C6H5O7) 100mM, hydroxyacetic acid (HOCH2COOH) 1%.With
Hydrochloric acid (HCl) adjusts pH value to 2, stirs 90min at 80 DEG C.Leaching operation reactor is 4 fixed bed reactors, using more
Grade interval counter-current extraction operating procedure；Pectin solution is obtained using plate filter filtering after leaching.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and concentration ratio is original solution body
Long-pending 30%, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, soaking time 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into jelly powder.
(9) polypentenol leaches
It extracts the filter residue obtained after pectin and leaches polypentenol, solid-liquid ratio 1:7, leaching temperature by leaching agent of petroleum ether
It is 75 DEG C, leaching time 120min；Leaching operation reactor is 4 fixed bed reactors, using multi-stage batch counter-current extraction
Operating procedure；Plate and frame filter press is collected by filtration filtrate, and filtrate carries out vacuum distillation concentration, distillation pressure 1,000-10,
000Pa, temperature are 50 DEG C of acquisition blackish green oily crude extracts；
(10) polypentenol crude extract hydrolyzes
Polypentenol crude extract uses 4% NaOH ethanol solution to be hydrolyzed for hydrolyzate, crude extract and hydrolyzed liquid
For product than being 1:5, hydrolysis temperature is 60 DEG C, hydrolysis time 120min, collects petroleum ether phase solution and carries out molecular distillation, distillation pressure
Power is 0.5-100Pa, 35 DEG C of cryosurface temperature, 60 DEG C of circulating water temperature, 70 DEG C of material heating temperature, 240 DEG C of vapo(u)rizing temperature, is received
Collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol ointment is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:5, so
After carry out silica gel column chromatography；Silica gel (100 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:10 (sample/
Silica gel), eluent is petrol ether/ethyl acetate mixed liquor, and ratio 8:2, eluting temperature is 30 DEG C, collects eluent and is subtracted
Pressure distillation, distillation pressure 1,000-10,000Pa, vapo(u)rizing temperature are 50 DEG C, obtain pale yellowish oil product.
(12) it calculates recovery rate: obtaining 76 grams of jelly powders.76 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is
7.6%.13 grams of ginkgolic acids are obtained, calculate 13 grams/1000 grams of recovery rate, obtaining recovery rate is 1.3%.
Comparative example 4:(traditional extraction liquid extracts pectin comparative experiments)
(1) picking of ginkgo fruit
Maturity period (fruit yellow, matter is soft, mature) picking in ginkgo is selected, is placed in ventilated environment and stores, strip
Exosper is spare.
(2) gingko episperm pre-processes
Weigh 1000 grams of gingko episperms, by screening removal go rotten, corruption raw material, will be selected after raw material rinse 3
There may be the impurity such as soil, sandstone, iron filings, wind to drench 10min, be crushed raw material using food masher for secondary removal.
(3) pectin leaches
The ratio of 1:10 adds leaching liquid, leaching liquid composition are as follows: sodium phosphate (Na into the raw material of crushing in mass ratio3PO4)
8%, pH value is adjusted to 2 with hydrochloric acid (HCl), stirs 90min at 80 DEG C.Leaching operation reactor is 4 fixed bed reactors,
Using multi-stage batch counter-current extraction operating procedure；Pectin solution is obtained using plate filter filtering after leaching.
(4) pectin solution decolourizes
Addition active carbon in pectin solution after filtration, and the 60min that decolourizes at 50 DEG C, pectin solution and active carbon
Ratio is 1L:15g.It is filtered after decoloration using plate filter.
(5) pectin solution is concentrated
Filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, and concentration ratio is original solution body
Long-pending 30%, ultrafiltration retaining molecular weight are 300,000, and operating pressure 0.1MPa, operation temperature is room temperature.
(6) pectin ethanol precipitation
95% ethanol solution is added in pectin solution after concentration, controls final concentration of 70% of ethyl alcohol in mixed liquor,
It stirs evenly, adjusts the pH value of mixed liquor to 3.5, stand completely rear filtering to be precipitated in 4 hours, obtain pectin crude extract.
(7) pectin crude extract purifies
Pectin crude extract is purified using ethyl alcohol immersion process, removes small molecule and oil-soluble impurities, concentration of alcohol are followed successively by
Dehydrated alcohol, 90% and 80%, soaking temperature are room temperature, and immersion elution time is 45min.
(8) pectin is dry
Pectin after purification is dried at 55 DEG C, is then comminuted into jelly powder.
(9) polypentenol leaches
It extracts the filter residue obtained after pectin and leaches polypentenol, solid-liquid ratio 1:5, leaching temperature by leaching agent of petroleum ether
It is 75 DEG C, leaching time 120min；Leaching operation reactor is 4 fixed bed reactors, using multi-stage batch counter-current extraction
Operating procedure；Plate and frame filter press is collected by filtration filtrate, and filtrate carries out vacuum distillation concentration, distillation pressure 1,000-10,
000Pa, temperature are 50 DEG C of acquisition blackish green oily crude extracts；
(10) polypentenol crude extract hydrolyzes
Polypentenol crude extract uses 4% NaOH ethanol solution to be hydrolyzed for hydrolyzate, crude extract and hydrolyzed liquid
For product than being 1:5, hydrolysis temperature is 60 DEG C, hydrolysis time 120min, collects petroleum ether phase solution and carries out molecular distillation, distillation pressure
Power is 0.5-100Pa, 35 DEG C of cryosurface temperature, 60 DEG C of circulating water temperature, 70 DEG C of material heating temperature, 240 DEG C of vapo(u)rizing temperature, is received
Collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol ointment is configured to solution with petroleum ether dissolution, and polypentenol ointment and petroleum ether volume ratio are 1:5, so
After carry out silica gel column chromatography；Silica gel (100 mesh) wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount 1:7 (sample/silicon
Glue), eluent is petrol ether/ethyl acetate mixed liquor, and ratio 8:2, eluting temperature is 30 DEG C, collects eluent and is depressurized
Distillation, distillation pressure 1,000-10,000Pa, vapo(u)rizing temperature are 50 DEG C, obtain pale yellowish oil product.
(11) it calculates recovery rate: obtaining 76 grams of jelly powders.76 grams/1000 grams of recovery rate are calculated, obtaining recovery rate is
7.6%.12 grams of ginkgolic acids are obtained, calculate 12 grams/1000 grams of recovery rate, obtaining recovery rate is 1.2%.
Claims (5)
1. a kind of gingko episperm pectin and polypentenol extracting method, which is characterized in that in turn include the following steps:
(1) picking of ginkgo fruit
Selection picks ginkgo in 7-9 month Chinese olive phase, and it is spare to strip exosper；
(2) gingko episperm pre-processes
Gingko episperm first pass around screening removal go rotten, corruption raw material, it is selected after starting material with water rinse 2-5 time, wind drench
Then 5-30min is crushed gingko episperm using food masher；
(3) pectin leaches
The ratio of 1:5-1:30 adds leaching liquid, leaching liquid solute composition are as follows: phosphorus into the gingko episperm of crushing in mass ratio
Sour sodium (Na3PO4) 2-8wt%, disodium hydrogen phosphate (Na2HPO4) 0.5-4wt%, sodium citrate (Na3C6H5O7) 10-100mM, hydroxyl
Guanidine-acetic acid (HOCH2COOH) 0.2-1wt%；Leaching liquid salt acid for adjusting pH value to 2-6；The stirring leaching 45- at 70-90 DEG C
120min；Leaching operation reactor is 3-8 fixed bed reactors, and operating procedure uses multi-stage batch counter-current extraction process；Leaching
Pectin solution is obtained using plate filter filtering after taking；
(4) pectin solution decolourizes
Active carbon, and the 30-120min that decolourizes under the conditions of 50-70 DEG C of temperature, fruit are added in step (3) filtered pectin solution
The ratio of sol solution and active carbon is 1L:5-20g；Filtering obtains pectin solution；
(5) pectin solution is concentrated
Step (4) filtered pectin solution is cooled to room temperature, and is concentrated using ceramic super-filtering film, liquor capacity is after concentration
The 20-50% of original solution volume before being concentrated, ultrafiltration retaining molecular weight are 10,000-300,000, operating pressure 0.05-
0.3MPa, operation temperature are room temperature；Obtain fructose concentrating liquid；
(6) pectin ethanol precipitation
The ethanol water of volumetric concentration 85-95% is added in step (5) fructose concentrating liquid, controls the whole body of ethyl alcohol in mixed liquor
Product concentration is 50%-80%, is stirred evenly, and adjusts the pH value of mixed liquor to 3-6, stands 0.5-4 hours completely rear mistakes to be precipitated
Filter, solid matter are the pectin crude extract obtained；
(7) pectin crude extract purifies
The pectin crude extract that step (6) obtains is purified using ethyl alcohol immersion process, and it is dense that concentration of alcohol is followed successively by dehydrated alcohol, volume
It spends 88-92% ethanol water and volumetric concentration 78-82% ethanol water, soaking temperature is room temperature, every section of soaking time is
30-90min；
(8) pectin is dry
Pectin after purification is dried at 50-70 DEG C, is then comminuted into pectin powder；
(9) polypentenol leaches
The filter residue that step (3) is obtained by filtration leaches polypentenol, solid-liquid ratio 1:5-1:10, leaching temperature by leaching agent of petroleum ether
Degree is 60-90 DEG C, leaching time 60-300min；Leaching operation reactor is 3-8 fixed bed reactors, using between multistage
It has a rest counter-current extraction operating procedure, the counter-current extraction refers to that material is flowed with leaching liquid at opposite direction, and material is anti-from left side
Answer device reactor flow to the right, leaching liquid is from right side reactor reactor flow to the left；Filter is collected by filtration in plate and frame filter press
Liquid, filtrate carry out vacuum distillation concentration, distillation pressure 1,000-10, and 000Pa, vapo(u)rizing temperature are 40-60 DEG C of acquisition blackish green
Oily crude extract；
(10) polypentenol crude extract hydrolyzes
The crude extract obtained in step (9) is the mixture of polypentenol He its acetic acid esters, it is necessary to acquisition polypenthylene be hydrolyzed
Alcohol, hydrolyzate are the NaOH ethanol solution of mass concentration 2-10%, and crude extract and hydrolyzate volume ratio are 1:5-20, hydrolysis temperature
It is 50-70 DEG C, hydrolysis time 30-240min collects petroleum ether phase solution and carries out molecular distillation, distillation pressure 0.5-
100Pa, 30-60 DEG C of cryosurface temperature, 50-90 DEG C of circulating water temperature, 40-80 DEG C of material heating temperature, vapo(u)rizing temperature 180-320
DEG C, collection evaporates excess, obtains dark-brown polypentenol extract；
(11) polypentenol purifies
Polypentenol extract is configured to solution with petroleum ether dissolution, and polypentenol extract and petroleum ether volume ratio are 1:2-5,
Then silica gel column chromatography is carried out；Silica gel 50-200 mesh wet method dress post is isolated and purified, chromatography condition are as follows: applied sample amount sample/silicon
Glue is 1:5-20, and eluent is petrol ether/ethyl acetate mixed liquor, and ratio 9:1-7:3, eluting temperature is 25-50 DEG C, is collected
Eluent is evaporated under reduced pressure, distillation pressure 1,000-10, and 000Pa, vapo(u)rizing temperature are 40-60 DEG C, obtains pale yellowish oil
Product.
2. gingko episperm pectin according to claim 1 and polypentenol extracting method, it is characterized in that: the step
(1) the Chinese olive phase of ginkgo is the 7-9 month；Step (2) gingko episperm first passes around mildew and rot, the corrupt raw material of screening removal,
There may be one of soil, sandstone, iron filings impurity or two kinds or more to prevent in gingko episperm raw material, after selected
Starting material with water rinses 2-5 times, and wind drenches 5-30min, is then crushed gingko episperm using food masher.
3. gingko episperm pectin according to claim 1 and polypentenol extracting method, it is characterized in that: the step
(3) leaching liquid solute preferably constitutes are as follows: sodium phosphate (Na3PO4) 3-5wt%, disodium hydrogen phosphate (Na2HPO4) 1-3wt%, lemon
Lemon acid sodium (Na3C6H5O7) 40-70mM, hydroxyacetic acid (HOCH2COOH) 0.4-0.7wt%.
4. gingko episperm pectin according to claim 1 and polypentenol extracting method, it is characterized in that: the step
(3) leaching operation reactor is the 3-8 fixed bed reactors successively contacted, and operating procedure uses interval counter-current extraction process,
The counter-current extraction process refers to that material and leaching liquid are flowed at opposite direction, and material is from left side reactor reactor to the right
Flowing, leaching liquid is from right side reactor reactor flow to the left；Pectin is obtained using plate filter filtering after leaching
Solution.
5. gingko episperm pectin according to claim 1 and polypentenol extracting method, it is characterized in that: the step
(4) pectin solution is using active carbon decoloring, and 50-70 DEG C of bleaching temperature, bleaching time 30-120min, pectin solution and active carbon
Ratio be 1L:5-20g；It is filtered after decoloration using plate filter.
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| CN1207311C (en) * | 2003-04-02 | 2005-06-22 | 石启田 | Ginkgo pectin extracted by using ginkgo external seed peel as raw material and extraction method |
| CN1234671C (en) * | 2004-08-11 | 2006-01-04 | 中国林业科学研究院林产化学工业研究所 | Molecular distillation purification method of polyprenol |
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